![Materials and methods
100% scoured & bleached cotton fabric
Diethylphosphatoethyltriethoxysilane (DPTS)
3-aminopropyltriethoxysilane (APTES)
1-hydroxyethane 1,1-diphosphonic acid
Melamine
Urea
Hydrochloric acid
Sodium hydroxide
Ethanol
N-hexakis-methoxymethyl- [1,3,5] triazine-2,4,6-triamine (MF)
Materials
Functional finishing of cotton fabric
APTES and DPTS were hydrolysed with HCl in deionized water,
vigorous stirring for 10 h at room temperature
55](https://image.slidesharecdn.com/seminarfin-191224094946/85/Sol-gel-technology-for-nano-textiles-55-320.jpg)
![Result and discussion 58
Diethylphosphatoethyltriethoxysilane (DPTS)
3-aminopropyltriethoxysilane (APTES)
N-hexakis-methoxymethyl- [1,3,5] triazine-2,4,6-triamine (MF)
Fig 17. TG curves of pure and treated cotton fabrics in nitrogen: Weight/% vs
Temperature/°C](https://image.slidesharecdn.com/seminarfin-191224094946/85/Sol-gel-technology-for-nano-textiles-58-320.jpg)
![59
Sample Residue at
360°C [%]
Residue at
750°C [%]
Untreated
cotton
14 2
DPTS 53 23
APTES 41 8
DPTS-APTES05 56 27
DPTS-APTES1 57 22
DPTS-APTES2 60 21
MF30 39 3
MF60 37 5
MF90 31 4
DPTS-MF1 60 20
DPTS-MF2 60 29
DPTS-MF3 60 33
Sample Total
burning
time [s]
Burning
Rate [mm/s]
Residue
[%]
Untreated
cotton
33 10 -
DPTS 35 6 37
APTES 24 7 33
DPTS-APTES05 21 10 60
DPTS-APTES1 20 9 48
DPTS-APTES2 24 8 53
MF30 150 10 27
MF60 51 12 19
MF90 28 8 20
DPTS-MF1 17 10 79
DPTS-MF2 19 8 68
DPTS-MF3 23 7 66
Table 6. Collected data of untreated
and treated fabrics by flammability
tests
Table 5. TGA data of untreated and
treated cotton fabrics in air
Diethylphosphatoethyltriethoxysilane (DPTS)
3-aminopropyltriethoxysilane (APTES)
N-hexakis-methoxymethyl- [1,3,5] triazine-2,4,6-triamine (MF)](https://image.slidesharecdn.com/seminarfin-191224094946/85/Sol-gel-technology-for-nano-textiles-59-320.jpg)
![60
Table 7. Flammability data
Sample Total burning time [s] Residue [%]
Untreated cotton 36 -
Only DPTS (O_D) 24 25
Only bisphosphonate (O_P) 23 10
Only melanine (O_M) 25 2.0
Only urea (O_U) 36 2.0
DPTS- bisphosphonate
combi (D_P)
38 40
DPTS- melamine combi
(D_M)
15 24
DPTS- urea combi (D_U) 25 22
Diethylphosphatoethyltriethoxysilane (DPTS)](https://image.slidesharecdn.com/seminarfin-191224094946/85/Sol-gel-technology-for-nano-textiles-60-320.jpg)
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Sol-gel technology for nano-textiles
- 1. 1 A seminar Sol-gel technologyfor nano-textiles Pratikhya Badanayak and Dr. Jyoti V. Vastrad
- 2. 2 Nanoparticles • 1 and100 nanometres (nm) in size can help make materials lighter, more durable, and more reactive. • Small size large surface area • Materials lighter • More durable • More reactive • Retain natural properties Why ?
- 3.
- 4. 4 Sol-Gel poly-condensation reactions Liquid state Gelstate 3D continuous network of the sol particles Stable dispersion of colloidal particles/ polymers
- 5. 5 Colloidal gel Polymergel Gels
- 6. 6 Reactions • Hydrogen cataion /hydroxideanaion Hydrolysis • Loss of water Condensation Hydrolysis M-OR + H2O = M-OH + ROH Condensation M-OH + M-OR = M-O-M + ROH M-OH + M-OH = M-O-M + H2O
- 7. 7 Mixing Gel formation Ageing Washing Drying Xerogel Aerogel Calcination Endproduct Cryogel Steps in sol-gel process
- 8. 8 Alcogel Xerogel AerogelCryogel
- 9. 9 • pH • Solvent •Temperature • Time • Catalyst • Agitation Factors affecting sol-gel process
- 10.
- 11. 11 Sol gel applicatio n intextile finishing Antibacte rial Anti- wrinkle Multifunc tional Flame retardant Water/oil /soil replant Self- cleaning Photo- catalytic UV- protectio n
- 12. 12 • Uniform &small sized • At low temperature- high density glass • Coating for films- easy • Objects or films with special porosity • Inorganic – organic composites • Fiber extraction Advantages of sol-gel process
- 13. 13 • Not used-industrially • Difficult- porosity • High permeability • Low wear-resistance • Weak bonding Dis-advantages of sol-gel process
- 14. Instruments for characterisation FourierTransform Infrared (FTIR) Spectra X- Ray Diffraction (XRD)
- 15. Transmission Electron Microscope (TEM) ScanningElectron Microscope (SEM)
- 16.
- 17.
- 18.
- 19. Synthesis and Characterizationof Sol–Gel Prepared Silver Nanoparticles • To investigate the effect of annealing temperature on the synthesis and characterisation of silver nanoparticles Ahlawat et al, 2014 19 Article - 1
- 20. Materials and methods Precursor AgNO3 TEOS Catalyst HNO3 Neutraliser NaOH Synthesisof silver–silica nanocomposites AgNO3 + water, constant stirring under gentle heating 15.5mL of ethanol + 22.5mL TEOS stirring for 25 min at room temperature Few drops of HNO3 and 10.5mL of water- stirred 20 Ageing -2 months Dried in vacuum at 600°C for 3 h
- 21. Characterisation techniques • XRD StructuralAnalysis • TEM Morphological studies • UV-Visible spectra Optical absorption spectra • FTIR Unknown material Heated at temperatures of 450°C and 550°C for half an hour 21
- 22. Result and discussion Fig1. (a) The XRD spectra of the 1.25 wt.% AgNO3 doped silica sample without calcination (b) The XRD spectra of the sample calcinated at 450°C for 30 min and (c) The XRD spectra of the 1.25 wt.% AgNO3 doped silica sample annealed at 550°C for 30 min 22 10.2 nm
- 23. Fig 2. (a)Absorption spectrum of AgNO3 doped silica samples without annealing and (b) Absorption spectrum of 1.41 wt.% AgNO3 doped silica samples annealed at 550°C for 30 min 23
- 24. Fig 3. (a)FTIR spectra of the 1.25 wt.% AgNO3 doped silica sample without calcination (b) FTIR spectra of the sample calcinated at 450°C for 30 min and (c) FTIR spectra of the sample annealed at 550°C for 30 min 24
- 25. 25 Fig 4. TheTEM image of the sample annealed at 550°C 8-25 nm
- 26. Conclusion 26 • Size- 10.2nm • Temperature- formation of nanoparticles • Size distribution- 8 nm to 25 nm spherical
- 27. Synthesis of zincoxide nanoparticles via sol-gel route and their characterization • To find a simple route to prepare nano ZnO particles via Sol- Gel method and characterize the final product using several techniques Alwan et al, 2015 27 Article - 2
- 28. Materials and methods 12.6gof zinc acetate dihydrate + 400 ml of double distilled water, continuous stirring 600 ml of absolute alcohol, stirring 6ml of H2O2 added, stirred and dried at 80℃ = nano zinc oxides Washed with double distilled water and dried at 80℃ in hot air oven Nano synthesis 28
- 29. Physical and Physico– chemical Characterization Morphology- SEM Crstallinity- XRD UV- Vis absorption- Spectro UV- VIS Double beam UVD-3500 Composition- FTIR 29
- 30. Result and discussion Fig5. XRD pattern of ZnO nanonanoparticls 30 58.3 nm
- 31. Fig 6. FTIRTransmition spectra of pure ZnO nanoparticls 31
- 32. Fig 8. UV-Visoptical absorption spectrum of ZnO nano particles Fig 7. Shows the SEM image of ZnO nanoparticles 32 100-200 nm
- 33. Conclusion 33 • Synthesis- successful •Spherical shape (100-200nm) • Uniform size
- 34.
- 35. Antibacterial activity ofcapsaicin-coated wool fabric • To encapsulate capsaicin to produce an antibacterial coating on wool fabrics by means of a sol-gel technique Liu et al, 2013 35 Article - 3
- 36. Materials and methods Substrate Doublejersey knitted interlock- 245 g/m2 Shrink proof- (chlorine/Hercosett℗) Coating Octyltriethoxysilane (OTES), 16 M 3-glycidoxypropyltrimethoxysilane (GPTMS), 16 M Ethanol , 160M and Water, 100M Tetraacetoxysilane (TAS), 1M- 30 min, 24 h Capsaicin 0.01 and 0.04 mol/l Wool - padded (one dip-and-nip, Werner Mathis Laboratory Pad Mangle) Air dried for 48 hours Control-I (without capsaicin) Control-II (uncoated original fabric) Washed - Hydropal at 45°C Fig 9. Structure of wool and Capsaicin 36
- 37. Characterisation and testing Opticaldensity- (UV-Vis) spectrophotometer Lower OD values indicate fewer bacteria Surface morphology SEM (LEO SEM S440, Germany) Antibacterial activities Gram-negative Escherichia coli (AATCC 11229, USA) Fourier transform infrared (FTIR) Burker Vertex 70 FTIR Spectroscope 37
- 38. Result and discussion Fig10. Fourier transform infrared (FTIR) spectra of wool fabric and capsaicin-sol-gel treated fabrics before and after laundry washes (Sol-Cap-UW: unwashed capsaicin sol-gel coated fabric, Sol-Cap-1 W: capsaicin sol- gel coated fabric-1 wash, Sol-Cap-3 W: capsaicin sol-gel coated fabric-3 washes, ATR: attenuated total reflectance) 38
- 39. Fig 12. Morphologyof untreated and coated fabrics and Escherichia coli after contact with fabrics Fig 11. (a) Fabric sample placed on five inoculums streaks (b) Heavy bacterial growth (arrow areas) underneath ‘control-I’ fabric (sol-gel coated) (c) No bacterial growth under capsaicin- coated fabric 39
- 40. Fig 13. Opticaldensity (OD) values of Escherichia coli cultures in soya broth medium incubated with fabric samples at different time intervals (Original: untreated fabric, Control-I: sol-gel coated without capsaicin, Fabric 1: coated with 0.01 mol/l capsaicin-sol gel, Fabric 2: coated with 0.04 mol/l capsaicin-sol gel) 40
- 41. Table 1. Antibacterialefficiency of capsaicin-coated wool fabric before and after washing Fabric sample Contact time (h) Bacteriagrowtha Antibacterial activity Original (Control-II) 24 Heavyb No effect Sol-coated (Control-I) 24 Moderate to heavy growthc Insufficient effect Capsaicin coated (Fabric 2) 24 No growthd Strong 1-wash (Fabric 2) 24 Slight growthe Limit of efficiency 3-wash (Fabric 2) 24 Slight growthe Limit of efficiency aThe growth of bacteria in the nutrient medium under fabric specimen bFull growth along streaks under the specimen cCompare to heavy, growth reduced to half dClear of bacteria growth eSlight growth compared to no growth 41
- 42. Conclusion 42 • (Silica- capsaicin)-Prolonged antibacterial effect • Reduced- antibacterial efficiency, capsaicin- attached
- 43. Simultaneous dyeing andanti-bacterial finishing of textile by sol-gel technique • To incorporate basic dyes and antimicrobial compound in the sol-gel coating of cotton and polyester cotton blend Kale et al, 2016 43 Article - 4
- 44. Materials and methods Material Plainweave cotton (12×17/cm) Plain weave polyester-cotton (P/C) Chemicals Tetraethylorthosilicate (TEOS) Glycidoxypropyltrimethoxysilane (GPTMS) Ethanol (98% pure) Hydrochloride acid (HCl) Cetyltriammoniumbromide (CTAB) Sodium Lauryl Sulphate Dye- Coracryl Violet C3R 44
- 45. Sample preparation • 50mlethanol, 34.20ml TEOS, 3.8ml Glycidoxypropyltrimethoxysilane (GPTMS) and 12ml HCl= 100ml • Magnetic stirrer for 24hours at room temperature • CTAB and 10 gpl Coracryl Violet C3R dye Sols • Padded- 2 dip 2 nip method with 70% expression for cotton and 60% for P/C • Air dried and cured in oven at 120°C for 1 hour • Soaped at 40°C for 2 hours by 10gpl Sodium Lauryl Sulphate at neutral pH • Washed and dried Application 45
- 46. Testing • Computer ColorMatching System (Spectra Scan 5100+) Colour strength • Wash, light and rubbing- ISO 105 C10, ISO 105-A02 and ISO 105 X-12 respectively Fastness • AATCC Test 100-2004 and the colony-forming units (CFUs) -Lapiz Coloney Counter Antibacterial activity • 10 wash cycles- with detergent (3% owf) at 40°C in a Rota dyer Wash Durability of Finish • Tensile strength and elongation- ASTM D 5034-95 • Stiffness-ASTM D1388-08(2012) Mechanical Properties Characterisation • SEM- JEOL JSM 6380LA, JEOL ltd. JapanSurface morphology 46
- 47. Result and discussion Fig14. Plot of Colour strength of the fabric samples 47 CATB
- 48. Conce ntratio n of CTAB (gpl) Cotton P/C Rubbing Fastness WashFastness Light Fastne ss Rubbing Fastness Wash Fastness Light Fastne ss Dry Wet Staini ng Colour Chang e Dry Wet Staini ng Colour Chang e 0 (Contr ol) 4-5 4 4-5 2 3-4 2-3 2 3 3 3-4 10 2 2-3 2-3 2-3 2-3 2 2-3 2-3 2-3 2-3 20 2 2-3 2 2-3 2-3 2 2-3 2 2-3 2-3 48 Table 2. Fastness properties for dyed and CTAB finished Cotton and P/C fabric with different concentration of CTAB
- 49. Conce ntrati on of CTAB (gpl) P/C Cotton BeforeWash After 10 washes Before Wash After 10 washes Number of Colonies after Reduc tion in coloni es (%) Number of Colonies after Reduc tion in coloni es (%) Number of Colonies after Reduc tion in coloni es (%) Number of Colonies after Reduc tion in coloni es (%) 0 hrs 24 hrs 0 hrs 24 hrs 0 hrs 24 hrs 0 hrs 24 hrs 0 (Contr ol) 0.30x 105 1.84x 105 Nil 0.92x 105 3.34x 105 Nil 1.53x 105 13.3x 105 Nil 1.73x 105 15.3x 105 Nil 10 2.73 x105 0.28 x105 89.74 3.67x 105 0.92x 105 74.93 2.00x 105 0.326 x105 83.7 3.52x 105 0.99x 105 71.88 20 2.20x 105 0.024 x105 98.80 3.98x 105 0.72x 105 81.91 1.63x 105 0.075 x105 95.3 2.09x 105 0.42x 105 78.46 Table 3. Antibacterial activity for dyed and CTAB finished fabric with CTAB for different concentration of CTAB against S.Aureus 49
- 50. Fig 15. Coloniesagainst S.aureus 50
- 51. Table 4. Mechanicalproperties of dyed and CTAB finished fabric for different concentration of CTAB Conce ntratio n of CTAB (gpl) P/C Cotton Tensile Strength (Kgf) Elongation (%) Bendin g Length (cm) Tensile Strength (Kgf) Elongation (%) Bending Length (cm)Warp Weft Warp Weft Warp Weft Warp Weft Untrea ted 119.7 63.3 59.7 32.5 1.19 63.9 33.36 11.46 17.07 2.57 0 (Contr ol) 117.8 52.8 52.1 32.6 1.21 57.7 30.55 14.21 19.23 2.64 10 116.8 51.5 54.5 35.2 1.23 56 29.04 15.47 19.87 2.71 20 115.8 50.43 55.7 36.1 1.53 53 24.63 16.10 20.04 2.81 51
- 52. Fig 16. SEManalysis 52
- 53. Conclusion 53 • Dyeing andanti-bacterial- successful • Fabric- soft
- 54. Phosphorus-Silica Sol-Gel HybridCoatings for Flame Retardant Cotton Fabrics • To investigates the use of organic-inorganic sol-gel coatings based on silica and phosphorous compounds for providing cotton fabrics with flame retardant features Rosace et al, 2017 54 Article - 5
- 55. Materials and methods 100%scoured & bleached cotton fabric Diethylphosphatoethyltriethoxysilane (DPTS) 3-aminopropyltriethoxysilane (APTES) 1-hydroxyethane 1,1-diphosphonic acid Melamine Urea Hydrochloric acid Sodium hydroxide Ethanol N-hexakis-methoxymethyl- [1,3,5] triazine-2,4,6-triamine (MF) Materials Functional finishing of cotton fabric APTES and DPTS were hydrolysed with HCl in deionized water, vigorous stirring for 10 h at room temperature 55
- 56. 56 3 Solutions containingthe MF were prepared by adding 0.002, 0.004 and 0.006 mol of MF (MF30, MF60, MF90 respectively) in deionized water Molar ratios of APTES (0.06, 0.12 and 0.25 M) and DPTS (0.25 M)- DPTS-APTES05, DPTS-APTES1 and DPTS-APTES2 In DPTS sol containing MF 0.002, 0.004 and 0.006 mol, DPTS-MF1, DPTS-MF2, DPTS-MF3 Cotton samples by a pad-cure-method (Werner Mathis padder) Dried at 80°C for 2 h, then cured at 150°C for 2 min in a laboratory oven
- 57. 57 Burning behaviour Flammability TesterModel 7633E ASTMD 1230 Thermogravimetric analyses TA Instruments Q500 thermobalance Characterisation
- 58. Result and discussion58 Diethylphosphatoethyltriethoxysilane (DPTS) 3-aminopropyltriethoxysilane (APTES) N-hexakis-methoxymethyl- [1,3,5] triazine-2,4,6-triamine (MF) Fig 17. TG curves of pure and treated cotton fabrics in nitrogen: Weight/% vs Temperature/°C
- 59. 59 Sample Residue at 360°C[%] Residue at 750°C [%] Untreated cotton 14 2 DPTS 53 23 APTES 41 8 DPTS-APTES05 56 27 DPTS-APTES1 57 22 DPTS-APTES2 60 21 MF30 39 3 MF60 37 5 MF90 31 4 DPTS-MF1 60 20 DPTS-MF2 60 29 DPTS-MF3 60 33 Sample Total burning time [s] Burning Rate [mm/s] Residue [%] Untreated cotton 33 10 - DPTS 35 6 37 APTES 24 7 33 DPTS-APTES05 21 10 60 DPTS-APTES1 20 9 48 DPTS-APTES2 24 8 53 MF30 150 10 27 MF60 51 12 19 MF90 28 8 20 DPTS-MF1 17 10 79 DPTS-MF2 19 8 68 DPTS-MF3 23 7 66 Table 6. Collected data of untreated and treated fabrics by flammability tests Table 5. TGA data of untreated and treated cotton fabrics in air Diethylphosphatoethyltriethoxysilane (DPTS) 3-aminopropyltriethoxysilane (APTES) N-hexakis-methoxymethyl- [1,3,5] triazine-2,4,6-triamine (MF)
- 60. 60 Table 7. Flammabilitydata Sample Total burning time [s] Residue [%] Untreated cotton 36 - Only DPTS (O_D) 24 25 Only bisphosphonate (O_P) 23 10 Only melanine (O_M) 25 2.0 Only urea (O_U) 36 2.0 DPTS- bisphosphonate combi (D_P) 38 40 DPTS- melamine combi (D_M) 15 24 DPTS- urea combi (D_U) 25 22 Diethylphosphatoethyltriethoxysilane (DPTS)
- 61. Conclusion 61 Hybrid phosphorus-silica nanosol • Thermal stability • Flame retardance
- 62.
- 63. Silk fabrics modificationby sol–gel method • To evaluate the potential of sol–gel hybrid coatings for the functionalization of silk fabrics • To improve their performances in terms of abrasion resistance Ferri et al, 2016 63 Article - 6
- 64. Materials and methods Sol-synthesis •Tetra-ethyl-ortho silicate (TEOS) • HCl Precursor Catalyst • 3-glycidoxypropyltrimethoxysilane, GLYMO • Hexadecyltrimethoxysilane, HDTMS • Octyltriethoxysilane, OctTEOS • 1H,1H,2H,2H-perfluorooctyltriethoxysilane, XF8 Alkyl/ fluro- alkyl functionlised Si-alkoxide • Water (Triton-X 100) or Isopropanol (stoichiometric water) Solvent (surfactant) • 20 min stirring- addition of functionlised alkoxide – stirring 4 hrs • pH= 2 Parameters 64
- 65. Composition of sols 65 3-glycidoxypropyltrimethoxysilane,GLYMO Hexadecyltrimethoxysilane, HDTMS Octyltriethoxysilane, OctTEOS 1H,1H,2H,2H-perfluorooctyltriethoxysilane, XF8
- 66. Fabric 54 g/m2 un-dyedtwill Silk Methods • Fabric stiffness- Hanging loop test • Abrasion resistance -James Heal (Halifax, UK) Mini-Martindale tester • Oil-repellency- UNI ENISO 14419.2010 • Tensile test- Universal Testing Machine 112 66
- 67. Result and discussion 0 5 10 15 20 Hanginglooptest - l -l0 Untreated S1 S2 S3 S4 S5 S6 S7 S8 S9 S10 Fig 18. Values of d=l-l0 from hanging loop test for untreated silk and coated fabrics 67 Isopropynol Water 3-glycidoxypropyltrimethoxysilane, GLYMO
- 68. Table 8. Abrasionresistance of treated samples Cycles 5000 7000 8500 S1 × × × S5 × × × S6 √ √ × S7 √ √ √ S8 × × × S9 √ √ √ S10 √ √ √ Fig 19. Appearance of samples after abrasion cycles: (a) untreated silk after 8500 cycles, (b) S1 after 2500 cycles, (c) S5 after 2500 cycles, (d) S6 after 8500 cycles, (e) S9 after 8500 cycles, and (f) S10 after 8500 cycles 68
- 69. Table 9. Staticcontact angles (α±3°) of oils drops on the S10 coated silk samples Degree OIL α (°) 1 Mineral oil 125 2 65:35 mineral oil: hexadecane 124 3 Hexadecane 121 4 Tetradecane 123 Fig 20. Maximum load and elongation at break (%) for coated silk fabrics samples * TT indicates the samples that were thermally treated at 100°C 69 144 146 148 150 152 Load at Break (N) Load at Break (N)
- 70. Conclusion 70 • Hybrid sol–gelsilica coatings- effective • Properties- some enhanced and some reduced
- 71. UV Photo-Stabilization ofTetrabutyl Titanate for Aramid Fibers via Sol–Gel Surface Modification • To investigate the effect of TiO2 coating on photo-stability of aramid fibers Xing and Ding, 2016 71 Article - 7
- 72. Materials and methods Preparationof TiO2 sols Precursor- Tetrabutyl titanate (TBT) Catalyst- HCl and Acetic acid Water Stirring for 10min at room temperature Materials and coating • 1.47 dtex Kevlar fiber- Tensile strength- 27.21 cN, Elongation at break -3.4% (DIN EN ISO 527-1-1996) Elastic modulus -648.7 cN/dtex • Dipped and treated at room temperature for 30 min and then dried and annealed in a vacuum oven at 80°C for 30min, then backed for 80°C & 500°C for 2 h. 72
- 73. Characterisation UV exposure conditionsPhoto-ageing procedures (UV lamp) for 24h Fiber tensile test Model XQ-1 fiber tester Microscopic analysis Composition (Crstalinity)- XRD Nanoscopic damage on the fiber surface- SEM Chemical composition- SCALAB MK-II X-ray Photo Electron Spectroscopy (XPS) 73
- 74. Result and discussion Fig21. XRD patterns of nanosized TiO2 baked at different temperatures for 2 h 74 25 nm
- 75. Fig 23. Tensilestrain of aramid fibers as a function of UV exposure time Fig 22. Tensile strength of aramid fibers as a function of UV exposure time 75
- 76. Fig 24. SEMimages of surface of aramid fiber. (a) Uncoated, exposure for 0 h (b) Uncoated, exposure for 156 h (c) Uncoated, exposure for 156 h (the latitudinal crack fracture) (d) Fiber fracture after tensile test, before exposure (e) Coated, exposure for 0 h (f) Coated, exposure for 156 h 76
- 77. Table 10. DeconvolutionAnalysis of C1s Peaks for Uncoated and Coated Aramid Fibers Sample Functional group ratio (%) C-C C=O COOH Uncoated fiber, 0 h 77.0 2.7 0 Uncoated fiber, 48 h 57.1 2.6 7.0 Uncoated fiber, 156 h 44.5 6.7 11.1 Coated fiber, 0 h 58.4 3.9 4.0 Coated fiber, 48 h 42.1 4.7 4.7 Coated fiber, 156 h 33.55 6.07 9.9 Table 11. XPS Spectra of Ti 2p Region for Coated Aramid Fibers with Various UV Exposures Sample Binding energy (eV) Ti 2p3/2 Ti 2p1/2 Gap Coated fiber, 0 h 458.4 464.0 5.6 Coated fiber, 48 h 458.9 464.5 5.6 Coated fiber, 156 h 459.2 464.9 5.7 77
- 78. Conclusion 78 • Coated fabric- •Photo stability • Protects- latitudinal cracks • Slow down- acylamide bond
- 79. Hemp Fibres Modificationby sol-gel Method for Polyolefin Composite Filling • To implement silica nanolevel coating on fibres surface without compromising the mechanical properties Zelca et al, 2017 79 Article - 8
- 80. Materials and methods •Precursor - TEOS- 0.09 to 0.14 M • Catalyst- HF- 0.8 to 1.6M • Solvent- Ethanol • Water Chemicals • Hemp stems • Hemp residue Material Nanosol variants, composition and post-processing temperature 80
- 81.
- 82. Result and discussion Fig25. SEM micrographs of hemp fibers modified by sol TEOS 0.09 M, HF 0.8 M (Sol variant a) Fig 26. EDX spectra of hemp fibers modified by sol TEOS 0.09 M, HF 0.8 M (Sol variant a) 82
- 83. Fig 27. SEMmicrographs of hemp fibers modified by sol TEOS 0.13 M, HF 0.8 M (Sol variant b) 83 Fig 28. EDX spectra of hemp fibers modified by sol TEOS 0.13 M, HF 0.8 M (Sol variant b)
- 84. Fig 29. SEMmicrographs and EDX spectra of hemp fibres modified by sol TEOS 0.14 M, HF 1.6 M (Sol variant c1) Fig 30. SEM micrographs of hemp residues modified by sol TEOS 0.14 M, HF 1.6 M (Sol variant c2) 84
- 85. Fig 31. Hempfibres 50 wt% composite Et, σmax, HV 85 Microhardness= HV Modulus of elasticity in tension= Et Tensile strength= σmax Surface
- 86. Conclusion 86 • Matrix-filler compatibility •Mechanical property • Better adhesion
- 87.
- 88. Statistical Optimization ofthe Sol–Gel Electrospinning Process Conditions for Preparation of Polyamide 6/66 Nanofiber Bundles • To statistically optimise the production and characterisation of polyamide 6/66 (PA 6/66) nanofiber obtained through sol-gel method Franco et al, 2018 88 Article - 9
- 89. Materials and methods •PA 6/66 • Solvent- Formic acid and acetic acid • Coagulation bath- Distilled water Materials • Conc- 12%wt, 17% wt, and 22% wt • Continuous stirring at room temperature Preparation of Polyamide Solutions • Voltage- 27.5 kV • Metal needle placed at 12 cm from the collector • Flow of the solution was controlled by a syringe pump Electrospinning Sol–Gel Process 89
- 90. Fig 32. Electrospinningsol–gel process • Nanofiber bundles of PA 6/66 , (12, 17, and 22%), following a unifactorial design completely random with 3 replicas and a significance level of α = 0.05 Statistical optimisation • Productivity in the deposit of nanofibers • Draw ratio • Nanofiber bundle tensile strength Variables 90
- 91. Phase transitions DSC ASTMD3418-08 Tensile strength EZ-Test L ASTM D3822 Morphology SEM JEOL JSM 6490 LV, Japan Characterisation techniques 91
- 92. Result and discussion Fig34. Draw ratio of the electrospinning sol–gel process Fig 33. Productivity of the basic electrospinning process 92
- 93. Fig 35. SEMimages of PA 6/66 electrospun nanofibers at different concentrations a) 12% wt., b) 17% wt., and c) 22% wt Fig 36. SEM images of polyamide 6/66 nanofiber bundles obtained through electrospinning sol–gel process at different concentrations a) 12% wt., b) 17% wt., and c) 22% wt 93
- 94. Samples Tg (°C)Tm (°C) ΔHm (J/g) Xc (%) PA 6/66 51.33 192.80 74.16 39.45 Nanofibers 17% 35.93 186.28 23.13 12.30 Nanofiber bundles 17% 40.29 190.79 33.47 17.80 Table 12. Thermal parameters obtained by DSC results 94 Fig 37. Tensile strength of polyamide 6/66 nanofiber bundles at different concentrations Glass-transition temperature (Tg) Melting temperature (Tm) Heat of fusion (ΔHm) Degree of crystallinity (Xc)
- 95. Conclusion 95 • 6/66 polyamideelectrospinning sol–gel process- (17% concentration) • High productivity • Better draw ratio • Good tensile strength
- 96.
- 97. Synthesis of aNovel Nanoencapsulated n-Eicosane Phase Change Material with Inorganic Silica Shell Material for Enhanced Thermal Properties through Sol-Gel Route • To develop a novel inorganic encapsulation technique for PCMs to enhance their performance in heat energy storage and thermal regulation • To investigate the formation mechanism of these silica nanocapsules Mohy et al, 2017 97 Article - 10
- 98. Materials and methods Tetraethyl orthosilicate Sodium silicate Hydrochloric acid n-Eicosane PEO-PPO- PEO Materials Synthesisof capsule 98 • TEOS/ Sodium silicate • W/O emulsion with HCl Hydrolysis/ condensation • PEO-PPO-PEO (0.25 g) was dissolved in 150 ml deionized water at 55°C, n-eicosane (15 g) stirred for 3 h • TEOS (15 g), HCl added- drop wise, stirred at 35°C • Silica-sol was added drop wise into the prepared emulsion and kept it stirring for 24 h TEOS derived nanoencapsul ation • PEO-PPO-PEO (0.5 g) was dissolved in 250 ml deionized water at 70°C, n-eicosane (10 g) stirred for 1 h • Sodium silicate (5 g), HCl added- drop wise, stirred at 35°C • Silica-sol was added drop wise into the prepared emulsion and kept it stirring for 24 h, heating 70°C Sodium silicate derived nanoencapsul ation • Washed- ethanol, dried at 50°C overnight Removal of sufactant
- 99. Fig 38. Schematicdiagram of nano-encapsulated n-eicosane PCM with silica shell via sol- gel process 99
- 100. Characterization Morphologies- Scanning ElectronMicroscope (SEM, SU1510) Fourier transform infrared (FTIR) spectra- Nicolet iS10 FT-IR spectrometer PCD- Differential Scanning Calorimetry instrument (DSC-Q200) Thermogravimetric analysis (TGA)- heating rate of 10°C/min 100
- 101. Fig 39. SEMimages of nanocapsules synthesized at different pH values and by using TEOS/sodium silicate as a silica-precursors: (a and b) n-eicosane/TEOS at pH 2.20; (c and d) n-eicosane/TEOS at pH 1.88; (e and f) n-eicosane/sodium silicate at pH2.94 101 Result and discussion
- 102. Fig 40. Particlesize distribution plots of the nanoencapsules synthesized at different pH values and silica precursors: (a,c,d) n-eicosane/TEOS; (b & e) n-eicosane/ sodium silicate 102
- 103. Fig 41. FTIRspectra of bulk and nanoencapsulated n-eicosane synthesized at different pH values and silica-precursors: (a) n-eicosane/TEOS; (b) n-eicosane/sodium silicate 103 Fig 42. DSC thermograms of the bulk and nanoencapsulated n-eicosane synthesized under different conditions, the curve numbers correspond to the samples code Samp le code N Eicosane/ Silica precursor ratio (wt/wt) pH 1 100/0 - 2 50/50 (TEOS) 2.25 3 50/50 (TEOS) 1.88 4 50/50 (TEOS) 2.2 5 50/50 (S.S) 2.94 6 50/50 (S.S) 2.5
- 104. Fig 43. Digitalphotographs: (a) n-eicosane/silica nanopasules; (b) pure n- eicosane heated at hot stage from room temperature to 60°C 104 Fig 44. TGA (a) and (b) DGA thermograms of silica-nanoencapsulated n-eicosane synthesized under different conditions, the curve numbers correspond to the samples code Samp le code N Eicosane/ Silica precursor ratio (wt/wt) pH 1 100/0 - 2 50/50 (TEOS) 2.25 3 50/50 (TEOS) 1.88 4 50/50 (TEOS) 2.2 5 50/50 (S.S) 2.94 6 50/50 (S.S) 2.5
- 105. Conclusion • Morphology- pHvalue • Nanoencapsulated n-eicosane (TEOS)- spherical morphologies at pH 2.20~2.30 • Good encapsulation efficeiency-TEOS • High encapsulation rate and heat stability- Sodium silicate 105
- 106. Reference 1. Ahlawat D.S., Kumari R., Rachana, Yadav I., 2014, Synthesis and characterization of sol-gel prepared silver nanoparticles. Int. J. Nanosci., 13(1): 1-8. 2. Alwan R. M., Kadhim Q. A., Sahan K. M., Ali R., Mahdi R., Kassim N. and Jassim A., 2015, Synthesis of zinc oxide nanoparticles via sol-gel route and their characterization. Nanosci. Nanotech., 5(1): 1-6. 3. Ferri L. D., Lorenzi A., Carcano E. and Draghi L., 2016, Silk fabrics modification by sol-gel method. Text. R. J., 88(1): 99-107. 4. Franco E., Dussan R., Amu M. and Navia D., 2018, Statistical optimization of the sol–gel electrospinning process conditions for preparation of polyamide 6/66 nanofiber bundles. Nanoscale Res. Letters, 671 (2018): 1-7. 5. Kale R., Agnihotri A. and Jagpat P. S., 2016, Simultaneous dyeing and anti-bacterial finishing of textile by sol-gel technique. Adv. App. Sci. Res., 7(2):116-122. 6. Liu X., Lin T., Peng B. and Wang X., 2012, Antibacterial activity of capsaicin-coated wool fabric. Text. R. J., 82(6): 584-590. 7. Mohy U. H. G, Jin Z. and Qufu W., 2017, Synthesis of a novel nanoencapsulated n-Eicosane phase change material with inorganic silica shell material for enhanced thermal properties through sol-gel route. J. Text. Sci. Eng., 7(2): 1-8. 8. Rosace G., Colleon C., Guido E. and Malucelli G., 2017, Phosphorus-silica sol-gel hybrid coatings for flame retardant cotton fabrics. Tekstilec, 60(1): 29-35. 9. Xing Y. and Ding X., 2016, UV photo-stabilization of tetrabutyl titanate for aramid fibers via sol–gel surface modification. J. App. Polymer Sci., 103(2016): 3113-3119. 10. Zelca Z., Kukle S. and Kajaks J., 2017, Hemp fibres modification by sol-gel method for polyolefin composite filling. Procedia Eng. 200 (2017): 26-32. 106
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Editor's Notes
- #15 Scanning Electron Microscope (SEM): The Scanning Electron Microscope (SEM) allows visualization of surface features of a solid sample by scanning through an electron beam. The treated and untreated test samples will be analysed under Scanning Electron Microscope. Fourier Transform Infrared Spectroscopy (FTIR): FTIR is a technique which is used to obtain an infrared spectrum of absorption or emission of a solid, liquid or gas. The surface functional group of treated samples will be examined using Fourier Transform Infrared Spectroscopy for assessing the functional properties.
- #17 UV-Vis spectrophotometer: UV-Vis is used to monitor the synthesis and stability of TiO2 and SiO2 nanoparticles. In UV-Vis, a beam with a wavelength varying between 180 and 1100 nm will be passes through the nano solution. The nano solution will absorbs the UV or visible radiation and the spectra of maximum absorption will be taken at different treatments. X-Ray diffraction (XRD): X-ray diffraction (XRD) is one of the most important non-destructive tools to analyze all kinds of matter ranging from fluids, to powders and crystals. The crystalline phase of the nanoparticles will be determined by using this. Scanning Electron Microscope (SEM)/ Transmission Electron Microscope (TEM): SEM/TEM allows visualization of surface features of a solid sample by scanning through an electron beam. The morphology of nanoparticles will be analysed under Scanning Electron Microscope or Transmission Electron Microscope. Dynamic Light Scattering (DLS): Dynamic light scattering (DLS) is a technique that can be used to determine the size distribution profile of small particles in suspension or polymers in solution. It works on laser diffraction method, where multiple scattering techniques will be employed to study the average particle size of the nanoparticles.
- #23 Braggs angle
- #56 diethylphosphatoethyltriethoxysilane (DPTS)
- #68 l- l0, l= loop length, l0= pear loop length, l-0.43l
- #73 Elastic modulus is a quantity that measures an object s resistance to being deformed elastically when stress is applied
- #78 XPS – x-ray photoelectron spectroscopy, acylamide bond breakage
- #84 Kev =
- #85 Thick coating, xerogel
- #86 Microhardness- material hardness when it is very small/ thin
- #94 Draw ratio – 12 and 22
- #95 Glass-transition temperature (Tg) Cystalinity – less free spaces, decrese interaction of molecular chain, low mobility, increse tg value
- #105 Thermogravemetric and derivative GA